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Lignin based phenolic resin and preparation and applications thereof

A phenolic resin and lignin-based technology, applied in the direction of aldehyde/ketone condensation polymer adhesives, adhesive types, adhesives, etc., can solve the problems of reduced curing temperature and shortened curing time of phenolic resins, and reduce the curing temperature , Reduce curing time, shorten the effect of curing time

Active Publication Date: 2019-06-07
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN106947419A discloses a phenolic resin adhesive synthesized by in-situ alkali lignin autocatalysis and its preparation method, and Chinese patent CN 106854264A discloses a preparation method of a rice husk-based lignin modified phenolic resin adhesive, although Both patents use lignin to modify phenolic resin, but the curing temperature of the prepared phenolic resin needs to be further reduced, and the curing time needs to be further shortened

Method used

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  • Lignin based phenolic resin and preparation and applications thereof
  • Lignin based phenolic resin and preparation and applications thereof
  • Lignin based phenolic resin and preparation and applications thereof

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0040] In this example, as a comparative example, 6 g of lignin and 9 g of phenol were added to a 500 mL three-necked flask and reacted in an oil bath at room temperature for 2 hours to obtain phenolated lignin. Then the phenol-formaldehyde ratio is 1:1.3, drop the formaldehyde with the constant pressure dropping funnel, first add 80% of the total amount of formaldehyde, and raise the temperature to 60°C for 1 hour. Then add the remaining 20% ​​formaldehyde and NaOH (NaOH is 4% of the lignin mass), and react at 80° C. for 2 hours to obtain a lignin-based phenolic resin.

[0041] Determination of the properties of the prepared lignin-based phenolic resin after being prepared into an adhesive shows that the free formaldehyde content is 0.25%, the bonding strength is 1.42MPa, the solid content is 48.46%, the free phenol content is 4.6%, and the viscosity is 324mPa. s.

Embodiment 2

[0043] Add 6g of lignin and 9g of phenol into a 500mL three-necked flask and react in an oil bath at room temperature for 2 hours to obtain phenolated lignin. Then the phenol-formaldehyde ratio is 1:1.3, drop the formaldehyde with the constant pressure dropping funnel, first add 80% of the total amount of formaldehyde, and raise the temperature to 60°C for 1 hour. Then add remaining 20% ​​formaldehyde, catalyst NaOH (NaOH is 4% of lignin quality) and catalyst molybdenum oxide nanoparticles (average particle diameter is 10nm, molybdenum oxide is 10% of the sum of NaOH and molybdenum oxide quality), at 80 Reaction at ℃ for 2h to obtain lignin-based phenolic resin.

Embodiment 3

[0045] The lignin-based phenolic resin was prepared according to the method of Implementation 2, except that the molybdenum oxide nanoparticles accounted for 30% of the total mass of the catalyst, and the average particle diameter of the molybdenum oxide nanoparticles was 50nm.

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Abstract

The invention relates to a preparation method of a lignin based phenolic resin. The preparation method comprises following steps: (1) reacting lignin with phenol at a temperature of 40 to 95 DEG C toobtain phenolated lignin after complete reactions; (2) dropwise adding formaldehyde into phenolated lignin to carry out reactions for 1 to 3 hours at a temperature of 40 to 95 DEG C; and (3) adding formaldehyde and a catalyst into the reaction product obtained in the step (2), and carrying out reactions for 1 to 2.5 hours at a temperature of 40 to 95 DEG C to obtain the lignin based phenolic resin; wherein the catalyst is composed of an alkali and nano particles, the nano particles are metal oxide nano particles, the nano particles account for 10 to 20% of the total weight of the catalyst, andthe particle size of the nano particles is 10 to 50 nm. The preparation method is environmentally friendly, the cost is low, and the prepared lignin based phenolic resin can be rapidly cured at a lowtemperature.

Description

technical field [0001] The invention relates to the technical field of phenolic resin preparation, in particular to a lignin-based phenolic resin and its preparation and application. Background technique [0002] Lignin is the main aromatic renewable resource, plays a role in supporting plant structure in plants, and is also an excellent alternative raw material for the preparation of polymers and chemicals. People obtain a large amount of lignin from biorefining industry, paper making industry, etc. However, the structure of lignin is still unclear, the chemical structure of lignin from the same source is not uniform, and the structure of lignin from different sources is inconsistent. Mainly used for fillers or additives, less for large-scale chemical production. [0003] The phenolic modification of lignin to prepare phenolic resin adhesives has gradually attracted people's attention. As an adhesive with excellent performance, phenolic resin is widely used in industrial ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C09J161/14
Inventor 石刚李赢赵云博王大伟桑欣欣白绘宇倪才华
Owner JIANGNAN UNIV
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